反应详情

温度

0 °C

To a solution of N2-tert-butylpyridine-2,3-diamine in dry DCM (150 mL) was added DIEA (17 mL, 95.5 mmol). The solution was cooled to 0° C. and carefully added 2,3-difluorobenzoyl chloride (8.35 g, 47.30 mmol). The reaction was allowed to warm up to RT and stirred for 1 hr. The mixture was then washed with water, saturated NaHCO3, and dried over MgSO4. Removal of the solvent by evaporation, the residue was purified by silica gel chromatography (5%-60% EtOAc/hexane) to yield N-(2-(tert-butylamino)pyridin-3-yl)-2,3-difluorobenzamide (4.0 g, 13.10 mmol); LC-MS m/e=306.1 (M+H).

1. temperatureto warm up to RT
2. washThe mixture was then washed with water, saturated NaHCO3
3. dry with materialdried over MgSO4
4. customRemoval of the solvent
5. customby evaporation
6. customthe residue was purified by silica gel chromatography (5%-60% EtOAc/hexane)